Author Topic: Update on Glacial Acid from Vinegar  (Read 2011 times)

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ADDkid

  • Guest
Update on Glacial Acid from Vinegar
« on: December 18, 2003, 01:21:00 PM »
I found the problem with using either sodium acetate or just distilling from vinegar. If you are using sodium acetate and concentrated sulfuric acid there will be water, little water, but still water.  The small amount of water is a big problem when distilling, and the point in which it comes over.

1.    If you are just distilling from vinegar, you are likely to get a boiling point of 103C, not matter how many times you distill.
2.   If you are using sodium acetate and sulfuric acid, and distilling you will first get a boiling point of 103c-105C, usually it will distill a little at 100c, and then reach 103c, which then proceeds very slowly to sustain 105c for most of the distillation.  When most of the solution has distilled, it may or may not climb to 110c, if it does reach 110c; it may or may not reach the 116c-118c, which is the boiling point of pure acetic acid, “Glacial acid”. It is find and dandy but, you only get a few mL.


The answer to the problem is so fucking easy that it pissed me off, because I did at least 20 distills which half where slow fractional distills. Anyway the problem is solved by using mass amount of magnesium sulfate; well at least until the solution is clear.  It can be tested by freezing it.  Water/acetic acids will not freeze in the Refig., but if you get a freeze in 10 mins, you know you have it pure.  I hope this information is useful, especially for those who like making there shit from scratch.
                                                                           ADDkid

Osmium

  • Guest
It miht help not to pour all the fractions...
« Reply #1 on: December 18, 2003, 02:31:00 PM »
It miht help not to pour all the fractions together for redistillation, and use a big long efficient column.


spectralmagic

  • Guest
Almost as masochistic as making your own GBL...
« Reply #2 on: December 18, 2003, 04:51:00 PM »
As Osmium says, collecting the fractions separately is a good idea...

It also helps to fuse the sodium acetate in the oven, converting the trihydrate to anhydrous (or close)...

Personally, after doing this a few times, I got fed up with the labour and mess involved, and just bought some...


gruns

  • Guest
I posted this elsewhere (and probably someone...
« Reply #3 on: December 18, 2003, 06:28:00 PM »
I posted this elsewhere (and probably someone before me), but I'm too lazy to find it, so here goes.   Supposedly, if you slowly drip cold vinegar over a chunk of crystallized acetic acid (in the fridge), the crystal will grow and the water will drain away.  I've never tried it though, I was about to then I found glacial in a store :p.


adroit_synth

  • Guest
seed crystal for glacial?
« Reply #4 on: December 23, 2003, 12:46:00 AM »
Supposedly, if you slowly drip cold vinegar over a chunk of crystallized acetic acid (in the fridge), the crystal will grow and the water will drain away.

SWIM has encountered this alleged procedure several times and can not see why it will not work as it has done so in many similar situations. Has anyone actually done this? SWIM would try right now but his lack of a GAA prohibits him.

adroit_synth

  • Guest
glacial crystalisation
« Reply #5 on: January 06, 2004, 08:09:00 PM »
C'mon guys! Somebee out there has had to try this. I have seen it a thousand times. I can't get it to work, but I suspect there is a reason like too dilute acetic or something.